HRID1076893
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 13.0 g (0.034 mole) of 2,7-bis(3-chloropropionyl)thioxanthene, 1 g of potassium iodide, 75 ml of diethylamine and 75 ml of tetrahydrofuran was allowed to stand for 72 hours and filtered. The residue was washed with tetrahydrofuran, evaporated to dryness then dissolved in ethanol. The solution was treated with ethanolic HCl, diluted with diethyl ether and the resulting solid was filtered off, recrystallized from methanol and diethyl ether and hydrated in a constant humidity chamber to give the desired product. M.P. 137°-140°C.
WORKUP
后处理
- filtrationfiltered
- washThe residue was washed with tetrahydrofuran
- customevaporated to dryness
- dissolutionthen dissolved in ethanol
- additionThe solution was treated with ethanolic HCl
- additiondiluted with diethyl ether
- filtrationthe resulting solid was filtered off
- customrecrystallized from methanol and diethyl ether and hydrated in a constant humidity chamber